HRID1285340

反应详情

EQUATION

反应方程式

HRID 1285340 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
18 °C

PROCEDURE

实验过程

92 g of 2-cyano 3-(2,6-dichlorophenyl)propenoic acid (Tetrahedron Lett., 1975, p.3643-4) are put into 860 ml of methanol and 285 ml of a 10% sodium hydrogen carbonate solution. This is cooled to 18° C. and the necessary quantity of sodium borohydride is introduced over a two and one-half hour period. The mixture is left for 2 hours at ambient temperature, then concentrated and acidified by adding 1N hydrochloric acid until a pH of 2.3. The solution is then extracted with ether and the organic layer is washed with water, dried on magnesium sulphate, filtered and evaporated. 82.4 g of 2-cyano 3-(2,6-dichlorophenyl)propanoic acid are obtained.

WORKUP

后处理

  1. concentrationconcentrated
  2. additionby adding 1N hydrochloric acid until a pH of 2.3
  3. extractionThe solution is then extracted with ether
  4. washthe organic layer is washed with water
  5. customdried on magnesium sulphate
  6. filtrationfiltered
  7. customevaporated